CN111233625A - Glycerol precipitation method in preparation of collagen peptide milk powder - Google Patents
Glycerol precipitation method in preparation of collagen peptide milk powder Download PDFInfo
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 title claims abstract description 127
- 238000000034 method Methods 0.000 title claims abstract description 76
- 239000000843 powder Substances 0.000 title claims abstract description 67
- 102000008186 Collagen Human genes 0.000 title claims abstract description 57
- 108010035532 Collagen Proteins 0.000 title claims abstract description 57
- 229920001436 collagen Polymers 0.000 title claims abstract description 57
- 235000013336 milk Nutrition 0.000 title claims abstract description 56
- 239000008267 milk Substances 0.000 title claims abstract description 56
- 210000004080 milk Anatomy 0.000 title claims abstract description 56
- 108090000765 processed proteins & peptides Proteins 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000001556 precipitation Methods 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000007788 liquid Substances 0.000 claims abstract description 37
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 235000005340 Asparagus officinalis Nutrition 0.000 claims abstract description 14
- 239000007787 solid Substances 0.000 claims abstract description 9
- 238000009835 boiling Methods 0.000 claims abstract description 6
- 238000007710 freezing Methods 0.000 claims abstract description 6
- 230000008014 freezing Effects 0.000 claims abstract description 6
- 238000002791 soaking Methods 0.000 claims abstract description 6
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 6
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 51
- 235000011187 glycerol Nutrition 0.000 claims description 47
- 239000000243 solution Substances 0.000 claims description 46
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 238000002156 mixing Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000012153 distilled water Substances 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000010998 test method Methods 0.000 claims description 10
- -1 alkyl glycoside Chemical class 0.000 claims description 8
- 229930182470 glycoside Natural products 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 5
- 244000269722 Thea sinensis Species 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- 238000004898 kneading Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 230000001376 precipitating effect Effects 0.000 claims description 5
- 239000012266 salt solution Substances 0.000 claims description 5
- 229920006395 saturated elastomer Polymers 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 230000009967 tasteless effect Effects 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 3
- 244000003416 Asparagus officinalis Species 0.000 claims 2
- 238000000926 separation method Methods 0.000 claims 1
- 241000234427 Asparagus Species 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 239000000344 soap Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 235000009508 confectionery Nutrition 0.000 description 3
- 239000003925 fat Substances 0.000 description 3
- 235000019197 fats Nutrition 0.000 description 3
- 238000007127 saponification reaction Methods 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- CMDGQTVYVAKDNA-UHFFFAOYSA-N propane-1,2,3-triol;hydrate Chemical compound O.OCC(O)CO CMDGQTVYVAKDNA-UHFFFAOYSA-N 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000019871 vegetable fat Nutrition 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
- C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
- C07K14/78—Connective tissue peptides, e.g. collagen, elastin, laminin, fibronectin, vitronectin, cold insoluble globulin [CIG]
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
Abstract
The invention discloses a glycerol precipitation method in preparation of collagen peptide milk powder, which comprises the following steps: s1, selecting fresh asparagus as a raw material, slicing, crushing by a crusher, putting into an ultrasonic extraction tank, adding water with the volume 10 times that of the fresh asparagus, soaking for 30 minutes, and boiling for 80-100 minutes by a conventional or high-pressure or ultrasonic method to obtain an extracting solution; s2, centrifuging the processed raw material by the extracting solution of S1 through a centrifuge; s3, adding 50-80% of emulsifier into the extracting solution of S2 according to dry matters, freezing the extracting solution into a solid state at low temperature, and directly subliming water in the solid state into a gas state without liquid state under vacuum so as to dehydrate the extracting solution to obtain collagen peptide milk powder; s4, detecting the collagen peptide milk powder obtained in the S3; thereby judging the quality of the prepared collagen peptide milk powder. The invention has simple components, cheap and easily obtained preparation apparatus, low production cost, simple preparation principle and easy popularization.
Description
Technical Field
The invention relates to the technical field of collagen peptide milk powder production, in particular to a glycerol precipitation method in preparation of collagen peptide milk powder.
Background
Glycerol, which is called glycerin by national standard, is colorless, odorless, sweet in taste, clear, viscous and liquid in appearance, and is an organic substance. Commonly known as glycerol. Glycerol, which absorbs moisture from the air, also absorbs hydrogen sulfide, hydrogen cyanide and sulfur dioxide. Insoluble in benzene, chloroform, carbon tetrachloride, carbon disulfide, petroleum ether and oils. Conventionally, glycerin has been recovered from by-products of soap production from animal and vegetable fats. To date, natural fats and oils are still the main raw materials for producing glycerin, with about 42% of natural glycerin being derived from a by-product of soap production and 58% being derived from fatty acid production. Saponification of fats and oils in the soap industry. The saponification reaction product was separated into two layers: the upper layer mainly contains fatty acid sodium salt (soap) and a small amount of glycerin, and the lower layer is waste alkali liquor which is a glycerin dilute solution containing salts and sodium hydroxide, generally containing 9-16% of glycerin and 8-20% of inorganic salt. And (3) grease reaction. The glycerol water (also called sweet water) obtained by hydrolyzing oil and fat has glycerol content higher than soap making waste liquid by 14-20% and inorganic salt 0-0.2%. In recent years, a continuous high-pressure hydrolysis method is generally adopted, a catalyst is not used in the reaction, the obtained sweet water generally does not contain inorganic acid, and the purification method is simpler than that of waste alkali liquor. The glycerol water obtained by hydrolyzing the grease or the soap making waste liquid contains low glycerol and various impurities, and the production process of the natural glycerol comprises the refining processes of purifying and concentrating to obtain crude glycerol, and distilling, decoloring and deodorizing the crude glycerol.
The existing glycerin preparation process has high cost, complex production process and expensive raw materials, so that the production cost is high, and therefore, a glycerin precipitation method for preparing collagen peptide milk powder is needed to solve the problems.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a glycerol precipitation method in the preparation of collagen peptide milk powder.
The invention provides a glycerol precipitation method for preparing collagen peptide milk powder, which comprises the following steps:
s1, selecting fresh asparagus as a raw material, slicing, crushing by a crusher, putting into an ultrasonic extraction tank, adding water with the volume 10 times that of the fresh asparagus, soaking for 30 minutes, and boiling for 80-100 minutes by a conventional or high-pressure or ultrasonic method to obtain an extracting solution;
s2, centrifuging the processed raw material by the extracting solution of S1 through a centrifuge;
s3, adding 50-80% of emulsifier into the extracting solution of S2 according to dry matters, freezing the extracting solution into a solid state at low temperature, and directly subliming water in the solid state into a gas state without liquid state under vacuum so as to dehydrate the extracting solution to obtain collagen peptide milk powder;
s4, detecting the collagen peptide milk powder obtained in the S3; thereby judging the quality of the prepared collagen peptide milk powder;
s5, mixing the collagen peptide milk powder of S3 with alcohol, then adding a sodium hydroxide solution, and separating out glycerol through a series of treatment processes.
Furthermore, the low temperature of the S3 is between-10 ℃ and-50 ℃, and the vacuum pressure is between 1.3 and 13 Pa.
Further, the step of separating out glycerol is as follows: mixing collagen peptide milk powder with 95% alcohol, adding 40% sodium hydroxide solution, and stirring and mixing with a glass rod; heating the obtained mixed solution in a water bath kettle for half an hour, and standing; adding distilled water into the prepared mixed solution, stirring and mutually dissolving to form viscous liquid, and adding saturated salt solution to separate out the glycerol.
Further, the mass ratio of the alcohol to the sodium hydroxide solution is 1: 2.
Further, the mixed liquid is contained in a beaker, water and alcohol are supplemented at any time in the heating process of the water bath kettle, and the mass ratio of the mixed liquid of the alcohol and the water is 1: 1.
Further, the mass ratio of the saline solution to the distilled water is 1: 7.
Further, the collagen peptide milk powder is powder.
Further, in step S3, the method for detecting the collagen peptide milk powder is one or more of a hand-pinching method, a nasal-smelling method, an eye-viewing method, a taste method, a skin test method, and the like.
Furthermore, the manual kneading method is to check that the powder is fine and smooth without impurities and any coarse and hard particles; the nasal smell method comprises checking no fishy smell and light fishy smell; the eye observation method comprises the operation steps of dissolving a proper amount of solvent, not sinking, rapidly dissolving at normal temperature, not precipitating and having good fluidity; the taste method is that the taste is light and nearly tasteless when the people drink the tea; the skin test method comprises the steps of taking a small amount of liquid to be coated on the back or face of a hand, and observing whether the liquid is completely absorbed or not after a moment, wherein the surface of the liquid has white crystals or foreign matter residues.
Further, the emulsifier adopts alkyl glycoside, and the variety of the alkyl glycoside is 0810, 0814, 1214, 0816, 1216, 1618 and the like, which are conventional types.
The invention has the following beneficial effects:
1. according to the invention, the fresh asparagus is used as the raw material, the raw material is simple and easy to obtain, the price is not high, the production cost is reduced, the energy consumption is low by heating in a water bath, the asparagus is prepared by mixing sodium hydroxide and alcohol and performing saponification reaction with collagen powder, the preparation principle is simple, the production process is simple, and the complicated operation is reduced.
2. The invention has simple component composition, cheap and easily obtained preparation apparatus, low production cost, simple preparation principle and easy popularization.
Drawings
FIG. 1 is a schematic diagram of a method for separating out glycerin during the preparation of collagen peptide milk powder according to the present invention;
FIG. 2 is a diagram of a detection method in a glycerin precipitation method in the preparation of a collagen peptide milk powder according to the present invention;
fig. 3 is a glycerin precipitation flow chart of the glycerin precipitation method in the preparation of collagen peptide milk powder of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When a component is referred to as being "connected" to another component, it can be directly connected to the other component or intervening components may also be present. When a component is referred to as being "disposed on" another component, it can be directly on the other component or intervening components may also be present. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Example 1:
referring to fig. 1 to 3, a method for separating out glycerin during preparation of collagen peptide milk powder includes the following steps:
s1, selecting fresh asparagus as a raw material, slicing, crushing by a crusher, putting into an ultrasonic extraction tank, adding water with the volume 10 times that of the fresh asparagus, soaking for 30 minutes, and boiling for 80 minutes by a conventional or high-pressure or ultrasonic method to obtain an extracting solution;
s2, centrifuging the processed raw material by the extracting solution of S1 through a centrifuge;
s3, adding 50% of alkyl glycoside of 0810 into the extracting solution of S2 according to dry matter, freezing the extracting solution into a solid state at low temperature, and directly subliming the water in the extracting solution into a gas state without passing through a liquid state under vacuum so as to dehydrate the extracting solution to obtain collagen peptide milk powder;
s4, detecting the collagen peptide milk powder obtained in the S3; thereby judging the quality of the prepared collagen peptide milk powder;
s5, mixing the collagen peptide milk powder of S3 with alcohol, then adding a sodium hydroxide solution, and separating out glycerol through a series of treatment processes.
Further, the low temperature of the S3 is-10 ℃, and the vacuum pressure is 1.3 Pa.
Further, the step of separating out glycerol is as follows: mixing collagen peptide milk powder with 95% alcohol, adding 40% sodium hydroxide solution, and stirring and mixing with a glass rod; heating the obtained mixed solution in a water bath kettle for half an hour, and standing; adding distilled water into the prepared mixed solution, stirring and mutually dissolving to form viscous liquid, and adding saturated salt solution to separate out the glycerol.
Further, the mass ratio of the alcohol to the sodium hydroxide solution is 1: 2.
Further, the mixed liquid is contained in a beaker, water and alcohol are supplemented at any time in the heating process of the water bath kettle, and the mass ratio of the mixed liquid of the alcohol and the water is 1: 1.
Further, the mass ratio of the saline solution to the distilled water is 1: 7.
Further, the collagen peptide milk powder is powder.
Further, in step S3, the method for detecting the collagen peptide milk powder is one or more of a hand-pinching method, a nasal-smelling method, an eye-viewing method, a taste method, a skin test method, and the like.
Furthermore, the manual kneading method is to check that the powder is fine and smooth without impurities and any coarse and hard particles; the nasal smell method comprises checking no fishy smell and light fishy smell; the eye observation method comprises the operation steps of dissolving a proper amount of solvent, not sinking, rapidly dissolving at normal temperature, not precipitating and having good fluidity; the taste method is that the taste is light and nearly tasteless when the people drink the tea; the skin test method comprises the steps of taking a small amount of liquid to be coated on the back or face of a hand, and observing whether the liquid is completely absorbed or not after a moment, wherein the surface of the liquid has white crystals or foreign matter residues.
Example 2:
referring to fig. 1 to 3, a method for separating out glycerin during preparation of collagen peptide milk powder includes the following steps:
s1, selecting fresh asparagus as a raw material, slicing, crushing by a crusher, putting into an ultrasonic extraction tank, adding water with the volume 10 times that of the fresh asparagus, soaking for 30 minutes, and boiling for 90 minutes by a conventional or high-pressure or ultrasonic method to obtain an extracting solution;
s2, centrifuging the processed raw material by the extracting solution of S1 through a centrifuge;
s3, adding 70% of alkyl glycoside of 0810 into the extracting solution of S2 according to dry matter, freezing the extracting solution into a solid state at low temperature, and directly subliming the water in the extracting solution into a gas state without passing through a liquid state under vacuum so as to dehydrate the extracting solution to obtain collagen peptide milk powder;
s4, detecting the collagen peptide milk powder obtained in the S3; thereby judging the quality of the prepared collagen peptide milk powder;
s5, mixing the collagen peptide milk powder of S3 with alcohol, then adding a sodium hydroxide solution, and separating out glycerol through a series of treatment processes.
Further, the low temperature of the S3 is-30 ℃, and the vacuum pressure is 5 Pa.
Further, the step of separating out glycerol is as follows: mixing collagen peptide milk powder with 95% alcohol, adding 40% sodium hydroxide solution, and stirring and mixing with a glass rod; heating the obtained mixed solution in a water bath kettle for half an hour, and standing; adding distilled water into the prepared mixed solution, stirring and mutually dissolving to form viscous liquid, and adding saturated salt solution to separate out the glycerol.
Further, the mass ratio of the alcohol to the sodium hydroxide solution is 1: 2.
Further, the mixed liquid is contained in a beaker, water and alcohol are supplemented at any time in the heating process of the water bath kettle, and the mass ratio of the mixed liquid of the alcohol and the water is 1: 1.
Further, the mass ratio of the saline solution to the distilled water is 1: 7.
Further, the collagen peptide milk powder is powder.
Further, in step S3, the method for detecting the collagen peptide milk powder is one or more of a hand-pinching method, a nasal-smelling method, an eye-viewing method, a taste method, a skin test method, and the like.
Furthermore, the manual kneading method is to check that the powder is fine and smooth without impurities and any coarse and hard particles; the nasal smell method comprises checking no fishy smell and light fishy smell; the eye observation method comprises the operation steps of dissolving a proper amount of solvent, not sinking, rapidly dissolving at normal temperature, not precipitating and having good fluidity; the taste method is that the taste is light and nearly tasteless when the people drink the tea; the skin test method comprises the steps of taking a small amount of liquid to be coated on the back or face of a hand, and observing whether the liquid is completely absorbed or not after a moment, wherein the surface of the liquid has white crystals or foreign matter residues.
Example 3:
referring to fig. 1 to 3, a method for separating out glycerin during preparation of collagen peptide milk powder includes the following steps:
s1, selecting fresh asparagus as a raw material, slicing, crushing by a crusher, putting into an ultrasonic extraction tank, adding water with the volume 10 times that of the fresh asparagus, soaking for 30 minutes, and boiling for 100 minutes by a conventional or high-pressure or ultrasonic method to obtain an extracting solution;
s2, centrifuging the processed raw material by the extracting solution of S1 through a centrifuge;
s3, adding 80% of alkyl glycoside of 0810 into the extracting solution of S2 according to dry matter, freezing the extracting solution into a solid state at low temperature, and directly subliming the water in the extracting solution into a gas state without passing through a liquid state under vacuum so as to dehydrate the extracting solution to obtain collagen peptide milk powder;
s4, detecting the collagen peptide milk powder obtained in the S3; thereby judging the quality of the prepared collagen peptide milk powder;
s5, mixing the collagen peptide milk powder of S3 with alcohol, then adding a sodium hydroxide solution, and separating out glycerol through a series of treatment processes.
Further, the low temperature of the S3 is-50 ℃, and the vacuum pressure is 9 Pa.
Further, the step of separating out glycerol is as follows: mixing collagen peptide milk powder with 95% alcohol, adding 40% sodium hydroxide solution, and stirring and mixing with a glass rod; heating the obtained mixed solution in a water bath kettle for half an hour, and standing; adding distilled water into the prepared mixed solution, stirring and mutually dissolving to form viscous liquid, and adding saturated salt solution to separate out the glycerol.
Further, the mass ratio of the alcohol to the sodium hydroxide solution is 1: 2.
Further, the mixed liquid is contained in a beaker, water and alcohol are supplemented at any time in the heating process of the water bath kettle, and the mass ratio of the mixed liquid of the alcohol and the water is 1: 1.
Further, the mass ratio of the saline solution to the distilled water is 1: 7.
Further, the collagen peptide milk powder is powder.
Further, in step S3, the method for detecting the collagen peptide milk powder is one or more of a hand-pinching method, a nasal-smelling method, an eye-viewing method, a taste method, a skin test method, and the like.
Furthermore, the manual kneading method is to check that the powder is fine and smooth without impurities and any coarse and hard particles; the nasal smell method comprises checking no fishy smell and light fishy smell; the eye observation method comprises the operation steps of dissolving a proper amount of solvent, not sinking, rapidly dissolving at normal temperature, not precipitating and having good fluidity; the taste method is that the taste is light and nearly tasteless when the people drink the tea; the skin test method comprises the steps of taking a small amount of liquid to be coated on the back or face of a hand, and observing whether the liquid is completely absorbed or not after a moment, wherein the surface of the liquid has white crystals or foreign matter residues.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A glycerol precipitation method in the preparation of collagen peptide milk powder is characterized by comprising the following steps:
s1, selecting fresh asparagus as a raw material, slicing, crushing by a crusher, putting into an ultrasonic extraction tank, adding water with the volume 10 times that of the fresh asparagus, soaking for 30 minutes, and boiling for 80-100 minutes by a conventional or high-pressure or ultrasonic method to obtain an extracting solution;
s2, centrifuging the processed raw material by the extracting solution of S1 through a centrifuge;
s3, adding 50-80% of emulsifier into the extracting solution of S2 according to dry matters, freezing the extracting solution into a solid state at low temperature, and directly subliming water in the solid state into a gas state without liquid state under vacuum so as to dehydrate the extracting solution to obtain collagen peptide milk powder;
s4, detecting the collagen peptide milk powder obtained in the S3; thereby judging the quality of the prepared collagen peptide milk powder;
s5, mixing the collagen peptide milk powder of S3 with alcohol, then adding a sodium hydroxide solution, and separating out glycerol through a series of treatment processes.
2. The method for separating out glycerin during the preparation of collagen peptide milk powder according to claim 1, wherein the low temperature of S3 is between-10 ℃ and-50 ℃ and the vacuum pressure is between 1.3 Pa and 13 Pa.
3. The method for separating out glycerin during the preparation of collagen peptide milk powder according to claim 1, wherein the step of separating out glycerin comprises: mixing collagen peptide milk powder with 95% alcohol, adding 40% sodium hydroxide solution, and stirring and mixing with a glass rod; heating the obtained mixed solution in a water bath kettle for half an hour, and standing; adding distilled water into the prepared mixed solution, stirring and mutually dissolving to form viscous liquid, and adding saturated salt solution to separate out the glycerol.
4. The method of claim 3, wherein the mass ratio of the alcohol to the sodium hydroxide solution is 1: 2.
5. The method of claim 3, wherein the mixture is filled in a beaker and water and alcohol are added at any time during the heating process in the water bath, and the mass ratio of the mixture of alcohol and water is 1: 1.
6. The method of claim 3, wherein the mass ratio of the saline solution to the distilled water is 1: 7.
7. The method of claim 1, wherein the collagen peptide milk powder is in a powder form.
8. The method of claim 1, wherein the collagen peptide milk powder is detected by one or more of a hand-pinching method, a nasal-smelling method, an eye-viewing method, a taste method, and a skin test method in step S3.
9. The method for glycerin separation in preparation of collagen peptide milk powder according to claim 8, wherein said manual kneading is to check that the powder is fine and free of impurities and any coarse and hard particles; the nasal smell method comprises checking no fishy smell and light fishy smell; the eye observation method comprises the operation steps of dissolving a proper amount of solvent, not sinking, rapidly dissolving at normal temperature, not precipitating and having good fluidity; the taste method is that the taste is light and nearly tasteless when the people drink the tea; the skin test method comprises the steps of taking a small amount of liquid to be coated on the back or face of a hand, and observing whether the liquid is completely absorbed or not after a moment, wherein the surface of the liquid has white crystals or foreign matter residues.
10. The method of claim 1, wherein the emulsifier is alkyl glycoside, and the alkyl glycoside is one of 0810, 0814, 1214, 0816, 1216, 1618, etc.
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Citations (3)
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CN102669673A (en) * | 2012-06-07 | 2012-09-19 | 秦皇岛长胜农业科技发展有限公司 | Asparagus collagen protein powder |
CN103319307A (en) * | 2013-06-27 | 2013-09-25 | 浙江工业大学 | Method for preparing sodium soap |
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